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1.
Matsumura Y Nishimura M Hiu H Watanabe M Kise N 《The Journal of organic chemistry》1996,61(8):2809-2812
Oxidative coupling of phenylacetic acid esters was easily achieved by treating the esters with TiCl(4) and then adding Et(3)N to the resulting solution. The products consisted of dl- and meso-2,3-diphenylsuccinic acid esters with the Claisen condensation product, and the ratio of these products depended on the reaction conditions. Reaction conditions suitable for high dl selectivity were determined, and a dimer of titanium enolate was postulated as an intermediate responsible for the high dl selectivity. The selectivities were compared with those in known oxidative couplings in which titanium enolate intermediates are prepared through lithium enolates and silyl enol ethers. The results suggest that the reactivities of titanium enolates intermediates depend on how they are generated. 相似文献
2.
A flexible and stereodivergent synthesis of the cis- and trans-fused 2,5-disubstituted octahydroquinolinone ring systems bearing all four stereogenic centers for the synthesis of the decahydroquinoline type of dendrobatid alkaloids has been achieved. The strategy involves stereoselective and stereodivergent construction of 2,3,6-trisubstituted piperidine ring systems using the Michael type of conjugate addition reaction to the enaminoesters 1 and 3, the intramolecular aldol type of cyclization reaction of keto aldehydes 11 and 12, and ring-closing metathesis of 21 as key steps. 相似文献
3.
Koichi Inoue Tasuku Sakamoto Yoshihito Fujita Saya Yoshizawa Maiko Tomita Jun Zhe Min Kenichiro Todoroki Kazuya Sobue Toshimasa Toyo'oka 《Biomedical chromatography : BMC》2013,27(7):853-858
Dexmedetomidine (Dex) is a selective central α2‐agonist with anesthetic properties and has been used in clinical practice for sedation in the intensive care unit (ICU) after operations. In this study, an analytical assay for the determination of Dex in a small amount of plasma was developed for the application to pediatric ICU trials. The quantification of Dex was constructed using the original stable isotope Dex‐d3 for electrospray ionization‐tandem mass spectrometry (ESI‐MS/MS) in the selected reaction monitoring mode. A rapid ultra‐performance liquid chromatography technique was adopted using ESI‐MS/MS with a runtime of 3 min. Efficacious concentration levels (50 pg/mL to 5 ng/mL) could be evaluated using a very small amount of plasma (10 μL) from patients. The lower limit of the quantification was 5 pg/mL in the plasma (100 µL). For sample preparation, a solid‐phase extraction was used along with the OASIS‐HLB cartridge type. Recovery values ranged from 98.8 to 100.3% for the intra‐ [relative standard deviation (RSD), 0.9–1.3%] and inter‐ (RSD, 0.9–1.5%) day assays. A stable test had recovery values that ranged from 97.8 to 99.7% with an RSD of 1.0–1.9% for the process/wet extract, bench‐top, freeze–thaw and long‐term tests. This method was used to measure the Dex levels in plasma from pediatric ICU patients. In the clinical ICU trial, the small amount of blood (approximate plasma volume, 200 μL) remaining from blood gas analysis was reused and targeted for the clinical analysis of Dex in plasma. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
4.
Evaluation of chemiluminescence reagents for selective detection of reactive oxygen species 总被引:2,自引:0,他引:2
Shinya Yamaguchi Kaname Ohyama Maiko Kohno Akira Takadate Naotaka Kuroda 《Analytica chimica acta》2010,665(1):74-27
In order to evaluate the chemiluminescence (CL) reagents for selective detection of reactive oxygen species (ROS), we comprehensively measured the CL responses of 20 CL reagents (three luminol derivatives, two imidazopyrazinone derivatives, eight lophine derivatives, six acridinium ester derivatives and lucigenin) against six types of ROS (superoxide anion: O2−, hydroxyl radical: OH, hydrogen peroxide: H2O2, hypochlorite anion: ClO−, singlet oxygen: 1O2, and nitric oxide: NO). As a result of the screening, it was found that nine CL reagents selectively detected O2− while one CL reagent selectively detected OH. However, no CL reagent had selectivity on the detection of H2O2, ClO−, 1O2 and NO. Our screening results could help to select the most suitable CL reagent for selective determination of different ROS.As an application study, 4-methoxyphenyl-10-methylacridinium-9-carboxylate (MMAC), one of the acridinium ester derivatives, showed high selectivity on the detection of O2−, and thus was applied to the assay of superoxide dismutase (SOD) activity. The dynamic range and detection limit of the developed CL assay were 0.1-10 and 0.06 U mL−1, respectively. Significant correlation (r = 0.997) was observed between the results by the CL assay using MMAC and the spectrophotometric assay using 2-(4-iodophenyl)-3-(4-nitrophenyl)-5-(2,4-disulfophenyl)-2H-tetrazolium monosodium salt. 相似文献
5.
Iwao Okamoto Mayumi Nabeta Misaki Yamamoto Maiko Mikami Tetsuya Takeya Osamu Tamura 《Tetrahedron letters》2006,47(40):7143-7146
An aromatic N-methyl amide containing N-(2-pyridyl) and 2,6-pyridinedicarboxamide moieties switches its conformation from cis to trans depending upon the acceptor number of solvents. 相似文献
6.
Masafumi UedaYuki Ikeda Aoi SatoYuta Ito Maiko KakiuchiHiroko Shono Tetsuya MiyoshiTakeaki Naito Okiko Miyata 《Tetrahedron》2011,67(25):4612-4615
A facile and practical synthesis of 3,5-disubstituted isoxazoles via a silver-catalyzed cyclization and subsequent protonation of alkynyl oxime ethers has been developed. The methodology was successfully applied to the synthesis of a biologically active isoxazolecarboxylic acid. 相似文献
7.
Kikura-Hanajiri R Kawamura M Miyajima A Sunouchi M Goda Y 《Analytical and bioanalytical chemistry》2011,400(1):165-174
In order to develop an analytical method for the discrimination of dextromethorphan (an antitussive medicine) from its enantiomer,
levomethorphan (a narcotic) in biological samples, chiral analyses of these drugs and their O-demethyl and/or N-demethyl metabolites in rat plasma, urine, and hair were carried out using LC-MS/MS. After the i.p. administration of dextromethorphan
or levomethorphan to pigmented hairy male DA rats (5 mg/kg/day, 10 days), the parent compounds and their three metabolites
in plasma, urine and hair were determined using LC-MS/MS. Complete chiral separation was achieved in 12 min on a Chiral CD-Ph
column in 0.1% formic acid–acetonitrile by a linear gradient program. Most of the metabolites were detected as being the corresponding
O-demethyl and N, O-didemethyl metabolites in the rat plasma and urine after the hydrolysis of O-glucuronides, although obvious differences in the amounts of these metabolites were found between the dextro and levo forms.
No racemation was observed through O- and/or N-demethylation. In the rat hair samples collected 4 weeks after the first administration, those differences were more clearly
detected and the concentrations of the parent compounds, their O-demethyl, N-demethyl, and N, O-didemethyl metabolites were 63.4, 2.7, 25.1, and 0.7 ng/mg for the dextro forms and 24.5, 24.6, 2.6, and 0.5 ng/mg for the
levo forms, respectively. In order to fully investigate the differences of their metabolic properties between dextromethorphan
and levomethorphan, DA rat and human liver microsomes were studied. The results suggested that there might be an enantioselective
metabolism of levomethorphan, especially with regard to the O-demethylation, not only in DA rat but human liver microsomes as well. The proposed chiral analyses might be applied to human
samples and could be useful for discriminating dextromethorphan use from levomethorphan use in the field of forensic toxicology,
although further studies should be carried out using authentic human samples. 相似文献
8.
Amaya T Hifumi M Okada M Shimizu Y Moriuchi T Segawa K Ando Y Hirao T 《The Journal of organic chemistry》2011,76(19):8049-8052
Oxosumanenes were synthesized through benzylic oxidation. The electronic and redox properties were revealed to exhibit the expanded π-conjugation compared to sumanene. Single-crystal X-ray analysis of monooxosumanene showed columnar π-stacking in a concave-convex fashion. Stereoselective trimethylation of the trioxo derivative was performed via 1,2-addition to the carbonyl groups. 相似文献
9.
10.
Dr. Masanori Shigeno Takuya Okawa Masaya Imamatsu Kanako Nozawa-Kumada Yoshinori Kondo 《Chemistry (Weinheim an der Bergstrasse, Germany)》2019,25(44):10294-10297
We herein demonstrate that the amide base generated in situ from CsF and N(TMS)3 catalyzes the deprotonative coupling reactions of terminal alkynes with polyfluoroarenes, wherein mono- and dialkynylations occur efficiently for penta- and hexafluorobenzenes, respectively. Tetraalkynylated products could also be synthesized from dialkynylated compounds. 相似文献